反应详情

温度

110 °C

Method K Combine 4-(6-nitro-1H-indol-3-yl)-benzonitrile, 9 (265 mg, 1.0 mmol), potassium phosphate tribasic (513 mg, 2.4 mmol), copper (I) iodide (38 mg, 0.2 mmol), and 2 mL of DMF in a 4 mL vial. Add 3-bromopyridine (120 μL, 1.2 mmol) and rac-trans-N,N′-dimethylcyclohexane-1,2-diamine (127 μL, 0.8 mmol). Warm the solution to 110° C. Let the solution stir overnight. Let the solution cool to RT, isolate the yellow precipitate by filtration, and wash the precipitate sequentially with DMF, 1:1 DMF:H2O, H2O, DMF, EtOAc, and then hexanes. Dry the precipitate under vacuum to yield 301 mg, 0.88 mmol, 88% of the title compound. LRMS (API ES+)=341.0 (M+H).

1. temperaturecool to RT
2. customisolate the yellow precipitate
3. filtrationby filtration
4. washwash the precipitate sequentially with DMF, 1:1 DMF
5. customDry the precipitate under vacuum